In This thesis P^N^P Pincer ligands, P^N^P a (aliphatic) and T -Ph (aromatic), and the corresponding Ni and Co complexes havebeensynthesized and characterized. These compound werecharacterized by single crystal X-ray diffraction, elemental analysis and different spectroscopies such as infrared (FT-IR), ultraviolet-visible spectroscopy (UV-Vis), 1 H, 3 1P NMR. The crystal structure bis[2-(diphenylphosphino)ethylamine]hydrochloride ( a ) and [Ni()Cl]Cl.EtOH, [Ni( a )Cl]Cl 2 .H 2 O complex were determined by single crystal X-ray diffraction. In addition, quantum mechanical calculations were performed on the thermodynamic and kinetic of the ligand preparation reaction, The effect of the different substitutio and solvent these reactions discussed.